Calorimetric bomb for the catalysis of ammonia



Jan. 28, 1930. G. clcALi 1,744,750

CALORIMETRIC BOMB FOR THE CATALYSIS OF AMMONIA Filed June '19. 1925 HZ-Did g k Y1 INVENTOR. {V G. Uzca III ATTORNEYS.

Patented Jan. 28, 1930 A UNITED; STATES PATENT oFFrcE GIOVANNI CICALI, OF BOLOGNA, ITALY, ASSIGNOR TO SOOIETA BREV'ETTI CICALI,

ANONIMA, OF PADOVA, ITALY, A JOINT-STOCK COMPANY CALORIMETRIC BOMB FOR THE OATALYSIS OF AMMONIA Application filed June 19, 1925, serial No. 38,386, and, in Italy February 16, 192.5.

This invention relates to a calorimetric bomb for the catalysis of ammonia which is illustrated in the accompanying drawing.

The calorimetric bomb for the catalysis of ammonia comprises a steel cylinder. 1 adapted to Withstand very high pressure and closed at both ends by firmly secured, gas tight plugs. The inner wall of the bomb is lined with heat insulating material 2 in order to minimize the transmission of heat to the bomb walls, the non-conducting lining being secured in place by the sheeting 3.

Inside of the bomb three coaxial cylinders are arranged, viz: an outer cylinder 5 of sheet metal, with open bottom end 6; a middle cylinder 6 with open top end 9, this cylinder consisting of sheets a, .2 spaced from each other, the spacing being filled with heat insulating material an inner cylinder 8 with 20 open bottom end 7, likewise of sheet metal and intended to contain the catalyzer 20. Between the cylinders 5 and 6 the coil 7 is arranged, the inside of the coil pipe being traversed by the gases From the catalyzer.

The connection between the catalyzer 20 and the coil 7 is secured through the cover 70 in which the top end of the coil is secured. The

opposite coil end is finally soldered to the connecting piece 1-. The gas tightness below.

is secured by the piece P and by the end plate It, the bottom plug pressing against these two parts. A pipe a is further provided, which supplies the bomb with the cold gases to be combined,viz hydrogen and nitrogen in the proportion required for forming ammonia. The pipe (1 being bifurcated, the gases can enter (through the cooks R and 1E, and through the inlet 0 and 0 the outer annular chamber cZ-d, while a portion of the cold gases can be conveyed through the cock it direct into the annular chamber 2', i. A pipe '0 and cock R, are further provided,

which permit to extract from the coil 7 a.

portion of the hot gases supplied by the catalyzer 20. From. the-external pipe E carrying the hot gases from the bomb, the

* gases are led by the branch pipe 13 to the water refrigerated condenser 14, and from this to the ammonia condenser 15, the outer,

surface of which is contacted with all of the ammonia produced and throttled at B, (after the second condensation). bined gases are led back through the tube T into circulation in very cold condition.

Working of the b0m? .-The high pressure cold mixture of hydrogen and nitrogen from a is delivered through the cocks R, 2 and pipes c, 0 into the bomb and passes through the annular chamber d, d maintaining at a low temperature the walls of the bomb resisting to the pressure. At the bottom of the bomb it enters at e the helical duct formed by the plates 5 and by the coil 7, where it gets heated through the heat given ofi' to it by the gases passing in downward direction inside of the coil. The mixture then enters through 9, g the annular chamber 2', 2 left between the catalyzer tube and the plate 2,

of cylinder 6. In the chamber 2', ithe mixture takes up heat from the catalyzer and comes into contact with the resistance 10, by which the gases are raised to combination temperature, this however is needed only during the starting period. The now suitably hot mix- The non-comture traverses the support S and reaches the catalyzer 20, in which a portion of the gases gets into combination and is transformed" into ammonia' At the top end of the catalyzer tube the gases enter the connecting duct K by which they are led into the coil 7. Here they give 01f heat to the gases that are passing in upward direction inside of the helical duct already mentioned and finally leave the bomb through the sleeve 1'.

An electric thermometer 12 shows the temperature variations taking place at the outlet from catalyzer.

In order to enable the regulating of th catalyzer temperature, that is to say, in order toprevent the catalyzer getting overheated, the pipe o and the cock R have been provided, by operating which latter a portion of the hot gases from the catalyzer can be conveyed direct to the condenser 14. The amount of hotgases traversing the coil 7 and giving off their heat to the freshly entering gases being thus lessened, the temperature of the gases leaving at g, g is lowered, and in this manner also the mixture temperature at the inlet of the catalyzer is lowered. Should the thermometer show an unduly high temperature so that an overheating of the catalyzer is to be feared, the whole or a portion of the cold mixture can be conve ed direct to the annular chamber 2', a throng the pipe at, the catalyzer being thus quickly restored into suitable, normal temperature conditions. The double regulation of the bomb is therefore obtained by suitably operating the cocks R and R The gases leaving the bomb through m and v are led to the water-cooled condenser 14 where, owing to the extraction of heat and 15 to the high pressure, a large proportion of the ammonia that has been formed is condensed, the residual ammonia being subsequently liquefied in the heat-exchange apparatus 15. The whole of the formed and condense ammonia descends through 8 into theflask 16. The heat exchange apparatus-15 is cooled by the ammonia vapours obtained by throttling (through cock R the passage of the liquid ammonia which has deposited at 5 the bottom of flask 16. Also the gases that have not combined and have consequently remained uncondensed go into the flask 16; these gases are very cold as they have passed through both condensers. These gases so through pipe T go to the circulation pump which sends them still cold to the synthesis. Through the cock R of the heat-exchange apparatus liquid ammonia, and through the cock R gaseous ammonia can be withdrawn.

Having now particularly described and ascertained the nature of my said invention and in what manner the same is to be performed, I declare that what I claim is 2- 1. In a calorimetric bomb for the high pressure catalysis of ammonia, a catalyst tube in the bomb, means for withdrawing gases from said tube, means for passing gases to said bomb in two streams, means for passing one of said streams in heat exchange relation with said tube, means for passing the other of'said streams in heat exchange relation with the wall of said bomb and with a portion only of the gases issuing from said tube, means for introducing said streams after said heat exchange into said tube.

2. In apparatus for the catalytic synthesis of ammonia, the combination, with acondensing device, of a catalyst bomb, a' tube therein to contain catalyst material, an inlet thereto for entering gases tobe treated,.an outlet for reaction products, means to divert a part of said reaction products, issuing'from said outlet, to the aforesaid condensin device, and means to divert another part of said no reaction products into heatexchange relationship with gases entering the bomb and prior to contact with the catalyst material.

GIOVANNI CICALI. 

